US7402261B2 - Slurry compositions, methods of preparing slurry compositions, and methods of polishing an object using slurry compositions - Google Patents
Slurry compositions, methods of preparing slurry compositions, and methods of polishing an object using slurry compositions Download PDFInfo
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- US7402261B2 US7402261B2 US11/205,029 US20502905A US7402261B2 US 7402261 B2 US7402261 B2 US 7402261B2 US 20502905 A US20502905 A US 20502905A US 7402261 B2 US7402261 B2 US 7402261B2
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- slurry composition
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- 239000000203 mixture Substances 0.000 title claims abstract description 245
- 239000002002 slurry Substances 0.000 title claims abstract description 219
- 238000005498 polishing Methods 0.000 title description 48
- 238000000034 method Methods 0.000 title description 27
- -1 glycol compound Chemical class 0.000 claims abstract description 85
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000002280 amphoteric surfactant Substances 0.000 claims abstract description 50
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 49
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 230000002378 acidificating effect Effects 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims abstract description 11
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004472 Lysine Substances 0.000 claims abstract description 11
- 239000004475 Arginine Substances 0.000 claims abstract description 10
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 claims abstract description 10
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims abstract description 10
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 claims abstract description 10
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims abstract description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 54
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 38
- 229910052721 tungsten Inorganic materials 0.000 claims description 38
- 239000010937 tungsten Substances 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 8
- 238000005260 corrosion Methods 0.000 claims description 8
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- ZKSGPMLZIPWJAF-ODZAUARKSA-N (z)-but-2-enedioic acid;oxalic acid Chemical compound OC(=O)C(O)=O.OC(=O)\C=C/C(O)=O ZKSGPMLZIPWJAF-ODZAUARKSA-N 0.000 claims description 3
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004343 Calcium peroxide Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 3
- ZJRXSAYFZMGQFP-UHFFFAOYSA-N barium peroxide Chemical compound [Ba+2].[O-][O-] ZJRXSAYFZMGQFP-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- LHJQIRIGXXHNLA-UHFFFAOYSA-N calcium peroxide Chemical compound [Ca+2].[O-][O-] LHJQIRIGXXHNLA-UHFFFAOYSA-N 0.000 claims description 3
- 235000019402 calcium peroxide Nutrition 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 239000001384 succinic acid Substances 0.000 claims 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 abstract description 3
- 229960003237 betaine Drugs 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 98
- 229910052751 metal Inorganic materials 0.000 description 62
- 239000002184 metal Substances 0.000 description 62
- 239000007800 oxidant agent Substances 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 30
- 230000008569 process Effects 0.000 description 18
- 235000012431 wafers Nutrition 0.000 description 14
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 10
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 9
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 9
- 239000011976 maleic acid Substances 0.000 description 9
- 238000007517 polishing process Methods 0.000 description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 9
- 230000007423 decrease Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 6
- 239000004471 Glycine Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000011800 void material Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000012258 stirred mixture Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003190 augmentative effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000001012 protector Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/7684—Smoothing; Planarisation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
Definitions
- the present invention relates to slurry compositions, to methods of preparing the slurry compositions, and to methods of polishing an object using slurry compositions.
- the slurry compositions and methods may be utilized in the fabrication of semiconductor devices.
- CMP Chemical mechanical polishing
- layers such as metal layers
- CMP processes are generally characterized by rotating a pad relative to the surface of a wafer with a slurry composition interposed there between. Chemical reaction between the slurry composition and materials of the wafer, coupled with mechanical polishing, result in the smoothing (planarizing) of surface features of one or more layers on the wafer.
- an oxide layer may be undesirably eroded as the result of differing polishing rates among various layers of the wafer, such as metal layers, barrier layers, insulating layers, and so on.
- an oxidizing agent it is known to add an oxidizing agent to the slurry composition in order to increase the polishing rate.
- the oxidizing agent can corrode the metal layer being polished, resulting in electrical disconnects with later formed metal layers. The result is often operational failure of the semiconductor device being fabricated.
- CMP slurry compositions are presented in U.S. Pat. No. 5,980,775, issued to Grumbine et al., and U.S. Pat. No. 5,958,288, issued to Mueller et al.
- these slurry compositions include peroxide as the oxidizing agent, and a metal catalyst for improving the oxidizing activity of the oxidizing agent in an effort to increase the polishing rate.
- Other examples are presented in U.S. Pat. No. 5,340,370, issued to Cadien et al., and U.S. Pat. No. 5,527,423, issued to Neville et al.
- These CMP slurry compositions generally include an unusually high amount of oxidizing agent in an effort to obtain a high polishing speed.
- the high concentration of oxidizing agent can cause problems. This is particularly true in the case of a metal layer, which can be etched and damaged by the conventional slurry composition. Further, voids can be disadvantageously formed in metal plugs by the oxidizing agent of conventional slurry compositions.
- FIGS. 1 and 2 are SEM images showing examples of damage to a metal layer that can result from a CMP process using a conventional slurry composition.
- FIG. 1 is a SEM image showing the metal layer damage that can be generated in the metal CMP process using a conventional SS W2000 slurry (trade name manufactured by Microelectronics Co., U.S.A
- FIG. 2 is a SEM picture showing the metal layer damage that can be generated in the metal CMP process using a conventional W slurry (trade name manufactured by Ceil Industries Inc., Korea).
- voids having diameters of about 900 ⁇ are observed at an upper portion of the metal layer.
- voids having diameters of about 600 ⁇ are observed at the upper portion of the metal layer. The presence of such voids increases the electrical resistance of the metal plugs, thus potentially causing operational failures.
- the metal layer in order to polish the metal layer with a constant polishing rate, it is desirable to maintain a constant concentration of the oxidizing agent.
- the oxidizing agent such as a peroxide compound
- the metal layer is not be polished at a constant polishing rate, and furthermore, the polishing rate is reduced as the polishing process proceeds.
- a slurry composition which include an acidic aqueous solution, an amphoteric surfactant, and a glycol compound.
- a slurry composition which includes an oxidizing agent, an abrasive, a carboxylic acid, an amphoteric surfactant, a glycol compound and pure water.
- a slurry composition which includes an oxidizing agent, an abrasive, a carboxylic acid, an amphoteric surfactant, a glycol compound, a pH-controlling agent and pure water.
- a slurry composition which includes an acidic aqueous solution and an amphoteric surfactant.
- a slurry composition which includes an acidic aqueous solution and a glycol compound.
- a method of preparing a slurry composition includes mixing an acid, an abrasive, a carboxylic acid and pure water to prepare a first mixture, adding a glycol compound and an amphoteric surfactant to the first mixture to prepare a second mixture, and adding a peroxide compound to the second mixture.
- a method of polishing an object includes preparing a slurry composition including an acidic aqueous solution, an amphoteric surfactant and a glycol compound, providing the slurry composition to a polishing pad, and polishing a surface of an object by contacting the polishing pad with the slurry composition against the surface of the object.
- FIGS. 1 and 2 are SEM pictures showing metal layer damage resulting from a CMP process using a conventional slurry composition
- FIG. 3 is a flow chart for explaining a method of preparing a slurry composition in accordance with an embodiment of the present invention
- FIG. 4 is a flow chart for explaining a method of polishing an object using a slurry composition in accordance with an embodiment of the present invention
- FIG. 5 is a graph illustrating the diameters of void generated in a metal layer relative to various wet etch rates.
- FIG. 6 is a graph illustrating the change in hydrogen peroxide concentration with an elapsed time after preparing a slurry composition.
- the slurry compositions of exemplary embodiments of the present invention include an acidic aqueous solution and one or both of an amphoteric surfactant and a glycol compound.
- the amphoteric surfactant may be adsorbed on a surface of the metal layer to form a protective layer which serves as a corrosion inhibitor for the metal layer.
- the protective layer may prevent or minimize contact between the oxidizing agent and the metal layer in the polishing process, thus preventing or minimizing damage to the metal layer which would otherwise be caused by the oxidizing agent.
- the amphoteric surfactant may also be adsorbed to surfaces of abrasive particles of the slurry, thus functioning as an agglomeration inhibitor of the abrasive. Accordingly, improved dispersion characteristics may result.
- amphoteric surfactant examples include a betaine compound and an amino acid compound. These can be used individually or in a mixture.
- Non-limiting examples of the amino acid compound include lysine, proline, and arginine. These can be used individually or in a mixture of two or more.
- the slurry composition When the slurry composition includes the amphoteric surfactant of less than about 0.0002 weight percent based on a total weight of the slurry composition, the slurry composition may not sufficiently protect against corrosion of the metal layer. On the other hand, when the concentration of the amphoteric surfactant in the slurry composition is greater than about 0.08 weight percent, the polishing rate may decrease, thereby deteriorating polishing efficiency. Therefore, the slurry composition preferably includes about 0.0002 to about 0.08 weight percent of the amphoteric surfactant based on the total weight of the slurry composition. The slurry composition more preferably includes about 0.002 to about 0.008 weight percent of the amphoteric surfactant.
- the glycol compound may improve the stability of the oxidizing agent. That is, for example, the oxidizing agent (e.g., hydrogen peroxide) of the slurry may easily decompose in water, thus reducing the oxidation power of the slurry composition.
- the glycol compound may reduce decomposition of the hydrogen peroxide to improve the stability of slurry composition and enhance the polishing efficiency.
- Non-limiting examples of the glycol compound include diethylene glycol, ethylene glycol, and polyethylene glycol. These can be used individually or in a mixture of two or more.
- the glycol compound is polyethylene glycol and a molecular weight of the polyethylene glycol in the slurry composition is greater than about 100,000, a viscosity of the slurry composition may be excessively augmented causing non-uniform polishing.
- the molecular weight of polyethylene glycol is preferably less than or substantially equal to about 100,000.
- the slurry composition of an embodiment of the invention preferably includes about 0.05 to about 10 weight percent of the glycol compound based on the total weight of the slurry composition.
- the slurry composition more preferably includes about 0.5 to about 1 weight percent of the glycol compound.
- the slurry composition of the present invention may include the amphoteric surfactant and/or the glycol compound so that the corrosion of the metal layer may be effectively prevented and also the stability of the oxidizing agent may be enhanced.
- the slurry composition includes the acidic aqueous solution so as to polish the object more efficiently.
- the acidic aqueous solution may include an oxidizing agent, an abrasive, a carboxylic acid and pure water.
- the slurry compositions of embodiments of the present invention may also include an oxidizing agent that may chemically oxidize a metal layer so that the chemically oxidized metal layer may be mechanically polished using an abrasive included in the composition.
- the oxidizing agent may include a peroxide compound and an acid.
- Non-limiting examples of the peroxide compound include hydrogen peroxide, benzoyl peroxide, calcium peroxide, barium peroxide, and sodium peroxide. These can be used individually or in a mixture of two or more.
- the slurry composition of the present embodiments preferably includes about 0.1 to about 10 weight percent of the peroxide compound.
- the slurry composition more preferably includes about 0.5 to about 5 weight percent of the peroxide compound.
- Non-limiting examples of the acid include nitric acid, sulfuric acid, hydrochloric acid, and phosphoric acid. These can be used individually or in a mixture of two or more.
- the slurry compositions of the present embodiments preferably includes about 0.001 to about 0.1 weight percent of the acid based on the total weight of the slurry composition.
- the slurry compositions more preferably include about 0.001 to about 0.05 weight percent of the acid.
- the slurry composition of the present embodiments may also include a carboxylic acid.
- the carboxylic acid may serve as an oxidizing agent stabilizer so that the polishing efficiency and the stability of the slurry composition may be improved.
- Non-limiting examples of the carboxylic acid include acetic acid, citric acid, glutaric acid, glycolic acid, formic acid, lactic acid, malic acid, maleic acid oxalic acid, phthalic acid, succinic acid, and tartaric acid. These can be used individually or in a mixture of two or more.
- the slurry composition of the present embodiments preferably includes about 0.01 to about 10 weight percent of the carboxylic acid based on the total weight of the slurry composition.
- the slurry composition more preferably includes about 0.1 to about 2 weight percent of the carboxylic acid.
- the slurry composition of the present embodiments may also include an abrasive.
- Non-limiting examples of the abrasive may include silica, alumina, ceria, zirconia, and titania. These can be used individually or in a mixture of two or more.
- the slurry composition of the present embodiments preferably includes about 0.1 to about 20 weight percent of the abrasive based on the total weight of the slurry composition.
- the slurry composition more preferably includes about 1 to about 7 weight percent of the abrasive.
- the slurry composition of the present embodiments may further include pure water.
- the slurry composition may include ultra pure water or deionized water.
- the slurry composition includes an oxidizing agent, an abrasive, a carboxylic acid, a pH-controlling agent, and pure water.
- the oxidizing agent, the abrasive and the carboxylic acid may be the same as those described previously.
- the pH-controlling agent is used to obtain a slurry composition having a suitable pH range.
- the metal layer being polished includes, for example, tungsten, aluminum, or copper
- the CMP process may be efficiently carried out in a pH of about 1 to about 6.
- the slurry composition has a pH of about 2 to about 4 in the case of tungsten, and a pH of about 4 to 6 in the cases of aluminum and copper.
- Non-limiting examples of the pH-controlling agent include potassium hydroxide (KOH) and tetramethylammonium hydroxide (TMAH).
- the slurry composition may include about 0.001 to about 1 weight percent of the pH-controlling agent based on the total weight of the slurry composition.
- the slurry composition includes an acidic aqueous solution and an amphoteric surfactant such as those described in detail previously.
- the slurry composition preferably includes, based on a total weight of the slurry composition, about 0.0002 to about 0.08 weight percent of the amphoteric surfactant, with all or a portion of the remainder being an acidic aqueous solution.
- the slurry composition more preferably includes about 0.002 to about 0.008 weight percent of the amphoteric surfactant.
- the slurry composition includes an acidic aqueous solution and a glycol compound such as those described previously in detail.
- the slurry composition preferably includes, based on a total weight of the slurry composition, about 0.05 to about 10 weight percent of the glycol compound, with all or a portion of remainder being the acidic aqueous solution.
- the slurry composition more preferably includes about 0.5 to about 1 weight percent of the glycol compound.
- FIG. 3 is a flow chart for explaining a method of preparing a slurry composition according to an exemplary embodiment.
- a first mixture is prepared by mixing an acid, an abrasive, a carboxylic acid with pure water in step S 10 .
- the first mixture may be advantageously prepared by stirring the acid, the abrasive, the carboxylic acid and the pure water for several minutes to several hours.
- the acid may include, for example, nitric acid, sulfuric acid, hydrochloric acid, or phosphoric acid.
- the abrasive may include, for example, silica, ceria, alumina, titania, or zirconia.
- the carboxylic acid may include, for example, acetic acid, citric acid, glutaric acid, glycolic acid, formic acid, lactic acid, malic acid, maleic acid oxalic acid, phthalic acid, succinic acid, or tartaric acid.
- the first mixture After pressurizing the first mixture, the first mixture may be provided into a disperser.
- a homonizer or an ultrasonic disperser may be used as the disperser.
- the disperser may disperse the first mixture by collisions of particles in the first mixture so that the disperser may improve a dispersibility of the first mixture. Accordingly, the abrasive in the first mixture may be dispersed homogeneously.
- the first mixture may be then filtered.
- a glycol compound and an amphoteric surfactant are added into the first mixture to form a second mixture in step S 12 .
- the glycol compound may include, for example, diethylene glycol, ethylene glycol, or polyethylene glycol.
- the amphoteric surfactant may include, for example, a betaine compound or an amino acid compound.
- the amino acid compound may include, for example, lysine, proline, or arginine.
- the second mixture may be sufficiently stirred for several minutes to several hours.
- the peroxide compound may include, for example, hydrogen peroxide, benzoyl peroxide, calcium peroxide, barium peroxide, or sodium peroxide.
- FIG. 4 is a flow chart for explaining a method of polishing an object according to another exemplary embodiment.
- a slurry composition including an acidic aqueous solution, an amphoteric surfactant and a glycol compound is prepared at step S 20 .
- the acidic aqueous solution may include a pH-controlling agent such as potassium hydroxide (KOH) or tetramethylammonium hydroxide (TMAH).
- KOH potassium hydroxide
- TMAH tetramethylammonium hydroxide
- the slurry composition is provided to a polishing pad at step S 22 , and then the surface of an object is polished by contacting the polishing pad with the surface of the object at step S 24 .
- the polishing pad and the object are rotated relative to each other.
- the polishing pad may rotate in a direction substantially identical to that of the object.
- the polishing pad may rotate along a direction substantially opposed to that of the object.
- the metal layer of the object may include a metal such as tungsten (W), aluminum (Al), titanium (Ti), tantalum (Ta), or copper (Cu).
- the object may be pressurized in the polishing process.
- the object may be chemically polished by the slurry composition, and also mechanically polished by rotating and pressurizing the object.
- an oxidizing agent such as a peroxide compound and an acid in the acidic aqueous solution may oxidize the metal layer to form a metal oxide film on the metal layer.
- the metal oxide film may then be mechanically polished by an abrasive such as silica, ceria, titania, alumina or zirconia in the acidic aqueous solution.
- the pH-controlling agent in the slurry composition may control a pH of the slurry composition relative to the metal included in the metal layer of the object so as to efficiently polish the object.
- the pH of the slurry composition may be in a range of about 1 to about 6. Particularly, when the object has the metal layer that includes tungsten, the pH of the slurry composition may be in a range of about 2 to about 4. When the object has the metal layer that includes copper or aluminum, the pH of the slurry composition may be in a range of about 4 to about 6.
- the slurry composition for polishing an object such as a semiconductor substrate will be further explained in accordance with various Examples and Comparative Examples.
- a slurry composition was prepared by mixing about 50 g of silica, about 20 g of hydrogen peroxide, about log of maleic acid, about 0.3 g of nitric acid, and about 4 g of lysine as an amphoteric surfactant with deionized water.
- Slurry compositions were prepared by performing processes substantially identical to that of Example 1 except for amphoteric surfactants.
- the amphoteric surfactants and contents of ingredients in the slurry compositions of Examples 2 and 3 are shown in following Table 1.
- Slurry composition was prepared by mixing about 50 g of silica, about 20 g of hydrogen peroxide, about 10 g of maleic acid, about 0.3 g of nitric acid, and about 0.8 g of diethylene glycol with deionized water.
- Each of slurry compositions of Examples 5 to 7 was prepared by mixing about 50 g of silica, about 20 g of hydrogen peroxide, about 10 g of maleic acid, about 0.3 g of nitric acid, about 0.8 g of diethylene glycol, and about 4 g of an amphoteric surfactant with deionized water.
- Types of amphoteric surfactants and contents of the amphoteric surfactants in the slurry compositions of Examples 5 to 7 are shown in Table 1 which is presented below.
- a conventional slurry composition was prepared.
- SS W2000 slurry composition (trade name manufactured by Cabot Microelectronics Co., U.S.A) was prepared.
- a slurry composition was prepared by mixing about 50 g of silica, about 20 g of hydrogen peroxide, about 10 g of maleic acid, and about 0.3 g of nitric acid with deionized water.
- a slurry composition was prepared by mixing about 50 g of silica, about 1.8 g of hydrogen peroxide, about 10 g of maleic acid, and about 0.3 g of nitric acid with deionized water.
- a slurry composition was prepared by mixing about 50 g of silica, about 20 g of hydrogen peroxide, about 10 g of maleic acid, about 0.3 g of nitric acid, and about 4 g of glycine with deionized water.
- a slurry composition was prepared by mixing about 50 g of silica, about 1.8 g of hydrogen peroxide, about 10 g of maleic acid, about 0.3 g of nitric acid, about 4 g of glycine, and about 0.8 g of diethyl glycol with deionized water.
- wet etch rates of tungsten layers were estimated according to variations in hydrogen peroxide concentrations in the slurry compositions.
- the slurry compositions were prepared by processes substantially identical to that of Comparative Example 2 except for the concentrations of hydrogen peroxide.
- the wet etch rates were estimated using blanket wafers that include tungsten layers, respectively.
- Oxide layers having thicknesses of about 1,000 ⁇ were formed on semiconductor substrates including polysilicon, and tungsten layers having thicknesses of about 10,000 ⁇ were formed on the oxide layers, thereby forming the blanket wafers.
- CMP processes were performed using the slurry compositions. After the CMP processes, sizes of voids generated in the tungsten layers were measured.
- FIG. 5 is a graph illustrating the diameters of the voids relative to the wet etch rate of the tungsten layer.
- the diameter of the voids generated in the tungsten layer are substantially proportional to the wet etch rate of the tungsten layer (an R 2 value is greater than about 99%).
- the wet etch rate of the tungsten layer may indirectly represent the diameter of the void generated in the tungsten layer. Accordingly, the size of the void may be estimated by measuring a wet etch rate of a metal layer using various slurry compositions.
- wet etch rates of tungsten layers were estimated using the slurry compositions according to Comparative Examples 1, 2 and 4, and Examples 1 to 3.
- the wet etch rates of the tungsten layers were estimated using blanket wafers including the tungsten layers. Oxide layers having thicknesses of about 1,000 ⁇ were formed on silicon substrates and the tungsten layers having thicknesses of about 10,000 ⁇ were formed on the oxide layers, thereby forming the blanket wafers.
- the slurry compositions according to Comparative Example 4 and Examples 1 to 3 were prepared as follows.
- the slurry composition of Comparative Example 2 was prepared by a process substantially identical to that of Example 1, whereas the amphoteric surfactant was not added into the slurry composition of Comparative Example 2.
- the blanket wafers were immersed into the slurry compositions, and then the wet etch rates of the tungsten layers were estimated by measuring the thicknesses of the tungsten layers relative to immersing time.
- the wet etch rates of the tungsten layers relative to the slurry compositions including amphoteric surfactants according to Examples 2 and 3 are remarkably lower than those of the tungsten layers relative to the slurry compositions according to Comparative Examples 1 and 2.
- the slurry composition including the amphoteric surfactant may effectively protect a metal layer such as the tungsten layer.
- the voids generated in the metal layer may be reduced by employing the slurry composition of the present embodiments in the CMP process for polishing a metal layer.
- the slurry composition according to Example 4 was prepared as follows. Firstly, about 50 g of silica, about 937.1 g of deionized water, about 10 g of maleic acid and about 0.3 g of nitric acid were stirred with about 2,000 rpm for about 2 hours in a flask to form a mixture. Subsequently, the stirred mixture was dispersed under a pressure of about 1,200 psi using a high-pressure dispersion process. About 0.8 g of diethylene glycol was added to the dispersed mixture and the mixture was additionally stirred for about 30 minutes. About 1.8 g of hydrogen peroxide was added into the mixture to prepare the slurry composition in accordance with Example 4. The slurry composition of Comparative Example 3 was prepared by a process substantially identically to that of Example 4, whereas diethylene glycol was not added into the slurry composition of Comparative Example 3.
- the stability of the oxidizing agent was estimated by measuring a concentration variation of hydrogen peroxide relative to time after preparing the slurry composition.
- FIG. 6 is a graph illustrating the concentration variation of hydrogen peroxide relative to time after preparing a slurry composition.
- the concentration of the hydrogen peroxide drastically decreases after preparing the slurry composition, and is reduced to less than about 50% after about 24 hours from preparing the slurry composition.
- the slurry composition includes the diethylene glycol as the stabilizer of the hydrogen peroxide, the hydrogen peroxide in the slurry composition has a relatively constant concentration as shown in FIG. 6 .
- the concentration of the hydrogen peroxide may be significantly stabilized by adding the glycol compound into the slurry composition. That is, the slurry composition according to exemplary embodiments may have a constant concentration of hydrogen peroxide, and the oxidizing power of the slurry composition may not decrease. As a result, a polishing rate of the metal layer may be maintained in the CMP process.
- a polishing rate of a metal layer such as a tungsten layer was estimated using the slurry compositions according to Comparative Examples 3 and 5, and Examples 5 to 7.
- the polishing rate of the tungsten layer is shown in Table 4 which is presented below.
- the polishing rate of the tungsten layer was estimated using blanket wafers including the tungsten layers. Each of the blanket wafers was prepared as follows.
- an oxide layer having a thickness of about 1,000 ⁇ was formed on a silicon substrate, and then a titanium nitride layer having a thickness of about 1,000 ⁇ was formed on the oxide layer. Subsequently, the tungsten layer having a thickness of about 10,000 ⁇ was formed on the titanium nitride layer.
- the slurry composition of exemplary embodiments includes an amphoteric surfactant as a protector of a metal layer. Particularly, since the amphoteric surfactant in the slurry composition may be adsorbed on a surface of the tungsten layer, an oxidation rate of the metal layer may be reduced, and the polishing rate of the metal layer may also decrease. However, the voids generated in the metal layer by the oxidizing agents may be effectively removed.
- the polishing rate of the metal layer further decreases so that the polishing rate of the metal layer using each of the slurry compositions of Examples 5 to 7 becomes lower than that of the metal layer using the slurry composition including the glycine according to Comparative Example 5.
- the slurry compositions of exemplary embodiments may effectively protect the metal layer including, for example, tungsten or aluminum, and simultaneously reduce the decrease of the polishing rate of the metal layer.
- a slurry composition may be used in a polishing process for an object such as a semiconductor substrate having a metal layer and/or an oxide layer.
- damage to the metal layer may be effectively prevented.
- the stability of an oxidizing agent in the slurry composition may be enhanced to thereby achieve a favorably constant polishing rate.
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KR102427981B1 (ko) * | 2013-10-23 | 2022-08-02 | 주식회사 동진쎄미켐 | 금속막 연마 슬러리 조성물 및 이를 이용한 금속막 연마 시 발생하는 스크래치의 감소 방법 |
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US9597768B1 (en) * | 2015-09-09 | 2017-03-21 | Cabot Microelectronics Corporation | Selective nitride slurries with improved stability and improved polishing characteristics |
KR101761789B1 (ko) * | 2015-12-24 | 2017-07-26 | 주식회사 케이씨텍 | 첨가제 조성물 및 이를 포함하는 포지티브 연마 슬러리 조성물 |
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US20030196386A1 (en) * | 2002-04-22 | 2003-10-23 | Jsr Corporation | Aqueous dispersion for chemical mechanical polishing |
US20050090106A1 (en) * | 2003-10-22 | 2005-04-28 | Jinru Bian | Method of second step polishing in copper CMP with a polishing fluid containing no oxidizing agent |
US20050236601A1 (en) * | 2004-04-21 | 2005-10-27 | Zhendong Liu | Barrier polishing solution |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20080057833A1 (en) * | 2006-08-30 | 2008-03-06 | Saint-Gobain Ceramics & Plastics, Inc. | Aqueous fluid compositions for abrasive slurries, methods of production, and methods of use thereof |
US7690968B2 (en) * | 2006-08-30 | 2010-04-06 | Saint-Gobain Ceramics & Plastics, Inc. | Aqueous fluid compositions for abrasive slurries, methods of production, and methods of use thereof |
Also Published As
Publication number | Publication date |
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JP2006060205A (ja) | 2006-03-02 |
CN1737885A (zh) | 2006-02-22 |
US20060060568A1 (en) | 2006-03-23 |
TWI375712B (en) | 2012-11-01 |
KR20060016498A (ko) | 2006-02-22 |
US8007676B2 (en) | 2011-08-30 |
US20080227296A1 (en) | 2008-09-18 |
TW200621955A (en) | 2006-07-01 |
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